I-Dodec-11-yn-1-ol (CAS# 18202-10-3)
I-Dodec-11-yn-1-ol (CAS# 18202-10-3) Ulwazi
ukulungiselela | I-NaH(7.5g, 60% ukuhlakazwa kwamafutha, 326mmol) yengezwe inqwaba ngenqwaba ku-dodecyl -3-alkyne -1-alcohol (10.0g,54.95mmol;GF Smith) esixazululo esinyakazisiwe esingu-0 ℃ se-ethylenediamine (40mL). Ngemuva kwehora elingu-1, izinga lokushisa likhuphukela ku-70 ℃. Ngemva kwamanye amahora angu-8, pholisa ingxube yokusabela ibe ngu-0°C, yeka ngokucophelela ngamanzi abandayo eqhwa (100mL), bese ukhipha nge-ether (3 × 60mL). Ukukhishwa kwe-ether okuhlanganisiwe kwagezwa ngamanzi (100mL). Ukugeza amanzi kwakhishwa emuva nge-ether (3 × 60mL). Izingcaphuno ze-organic ezihlanganisiwe zagxiliswa ngaphansi kwe-vacuum, futhi izinsalela zafakwa ngaphansi kwekholomu ye-chromatography kusetshenziswa u-10% we-EtOAc/hexane ukuze zithole i-11-dodecyne -1-alcohol (7.4g,74%) engcoliswe ngo-3-5% wezinye isomers zesifunda ( i-regioisomer). TLC:30% EtOAc/hexane, Rf ≈ 0.4;1H NMR(300MHz,CDCl3)δ3.66(t,2H,J = 7.3Hz), 2.14-2.21(m,2H),1.93(t,J = 1.9Hz) ,1H),1.20-1.63(m,16H). |
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